EP3052223B1 - Composition pour la formation d'une membrane à base biologique, procede d'application sur des surfaces et utilisation de celle-ci - Google Patents

Composition pour la formation d'une membrane à base biologique, procede d'application sur des surfaces et utilisation de celle-ci Download PDF

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EP3052223B1
EP3052223B1 EP14790758.8A EP14790758A EP3052223B1 EP 3052223 B1 EP3052223 B1 EP 3052223B1 EP 14790758 A EP14790758 A EP 14790758A EP 3052223 B1 EP3052223 B1 EP 3052223B1
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composition
nanoparticles
concrete
bio
amount
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EP3052223A2 (fr
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Eduardus Aloysius Bernardus Koenders
Jure ZLOPASA
Stephen James Picken
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Technische Universiteit Delft
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Technische Universiteit Delft
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D105/00—Coating compositions based on polysaccharides or on their derivatives, not provided for in groups C09D101/00 or C09D103/00
    • C09D105/04—Alginic acid; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
    • C04B41/48—Macromolecular compounds
    • C04B41/4803—Polysaccharides, e.g. cellulose, or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D105/00—Coating compositions based on polysaccharides or on their derivatives, not provided for in groups C09D101/00 or C09D103/00
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D105/00—Coating compositions based on polysaccharides or on their derivatives, not provided for in groups C09D101/00 or C09D103/00
    • C09D105/06—Pectin; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
    • C04B2111/00293—Materials impermeable to liquids
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/24—Sea water resistance
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/25—Graffiti resistance; Graffiti removing
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/74—Underwater applications
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica

Definitions

  • the present invention is in the field of a composition for forming a bio-compatible membrane applicable to building material, such as concrete, cement, etc., to a method of applying said composition for forming a bio-compatible membrane and use of the composition for improving setting of concrete, protecting concrete or cement from degradation and as an anti-graffiti coating.
  • Concrete is a composite construction material composed primarily of aggregate, cement and water, with mortar being similar thereto, however using finer aggregates.
  • the aggregate is generally a coarse gravel or crushed rocks such as limestone, or granite, along with a fine aggregate such as sand.
  • the cement commonly Portland cement, and other cementing materials such as fly ash, blast furnace slag cement, ground calcium carbonate, etc. serve as a part of binder for the aggregate. Typically further additives are present.
  • Admixtures are ingredients other than water, fine aggregates, (hydraulic) cement, and fibers that are added to the concrete batch immediately before or during mixing, in order to change certain characteristics of the concrete, when set.
  • a sheet does typically not fully cover concrete.
  • a sheet may also be somewhat difficult to apply, especially when concrete is curved it is difficult to access, such as in high buildings and hidden areas, it may be of temporary nature, it can not be fully integrated with an underlying material, permeability may be difficult to adapt, toxic chemicals and solvents may be used, diffusion of membrane or constituents into concrete may take place, they may be sensitive with respect to time of application, typically they are non-degradable, and they may not be environmentally friendly.
  • a (semi)permeable membrane relates to a partially permeable membrane or a differentially permeable membrane.
  • a membrane allows certain molecules or ions to pass through it by diffusion, such as gaseous species. It is noted that a rate of passage depends on various parameters, such as pressure difference, concentration difference, and temperature difference between circumstances on either side of a membrane, and permeability of the membrane to a given species, which permeability depends on solute or species size, solubility, chemistry, etc.
  • US4316833 recites a liquid system containing no water to form an underground waterproof coating material containing a high concentration (70%+) of bentonite (sodium montmorillonite) which is non-hydrated, non-emulsifiable, unexpanded, non-jelled, non-thixotropic but is sufficiently liquid to be applied to a wood, metal or concrete substrate by a caulking gun, trowel or spray method. It can be used over a wide range of temperatures and can be applied to damp surfaces.
  • the invention relates to a bentonite based composition for coating walls or sealing joints in concrete, and sealing around pipe openings and the like in building construction.
  • the composition can be used for any type of waterproofing or water stop application if desired.
  • the system may comprise beads, which beads may be coated with Ca-alginate. From the above it is clear that the system has no capability to form a membrane; it is solely intended to swell. Application is therefore inside cracks and the like, in order to seal.
  • CN101502868 (A ) recites a centrifugal casting radiant tube coating and a preparation method thereof, the coating comprises the ingredients (mass percent) of: amongst others 25-30% of diatomite of, 5-10% of zircon powder, 4.5-5.0% of sodium bentonite, 2.0-2.5% of polyvinyl alcohol, 0.8-1.0% of sodium alginate, 3.5-4.0% of silica sol, and 46.82-49.95% of water, wherein, the mass percent of the diatomite and the zircon powder is not less than 35% and not more than 37%, the mass percent of titanium powder and iron powder is not less than 2.7% and not more than 2.9%, and the mass percent of the sodium bentonite plus the polyvinyl alcohol plus the sodium alginate is not less than 8.0% and not more than 8.2%.
  • the coating is used for the centrifugal casting radiant tube after dry-blending, mixed grinding and sieving, uniformly distributed bulges (namely pitting surface) can be formed on the outer surface of the radiant tube to improve heat efficiency of the radiant tube.
  • the coating also has excellent adhesive force, high temperature strength and crack resistance, thus reducing defects on the surface of the radiant tube and improving quality of complex tube.
  • the present invention relates to a composition for forming such a membrane and use thereof which overcomes one or more of the above disadvantages, without jeopardizing functionality and advantages.
  • the present invention relates to an aqueous composition for forming a bio-compatible membrane, a method for forming a bio-compatible flexible membrane,.
  • the invention makes use of non-toxic and environmentally friendly components. These components are biocompatible, i.e. an impact on the biological environment is considered minimal.
  • the composition has as a main liquid water, or may be formed primarily from water.
  • the polymer used is bio-degradable, that can be degraded by e.g. bacteria, yet is stable enough to provide e.g. a good protection for an underlying material, such as concrete.
  • the polymer dissolves sufficiently in water, typically forming a viscous solution.
  • the polymer is capable of forming a gel, once being in contact with polyvalent cations, thereby forming a flexible, impermeable membrane.
  • the membrane preserves water being present in an underlying material and protects the underlying material from the environment. Certain types of polymers used may form a recoverable coating or membrane, .
  • the polymer provides a conformal coating to a surface to which it is applied.
  • the coating acts e.g. as protection against chemicals, moisture, dust, and temperature extremes that, if uncoated (non-protected), could result in damage or failure of an underlying surface/material, and also maintains conditions of the surface, such as humidity or moisture content.
  • a silicate provides a more stiff coating, the polymer a more flexible coating, and a combination of silicate and polymer may have in between characteristics.
  • the present composition does not or at the most to a small extent penetrate into a surface to which it is applied.
  • the membrane or coating formed can not be washed away by water, such as by rain.
  • the membrane is fully integrated with an underlying surface, adheres thereto, and may be considered as a layer having suitable characteristics. So surprisingly the present composition may be applied directly to a surface and provides advantageous effects.
  • Platelet nanoparticles have dimensions wherein a length, and likewise a width, thereof is significantly larger than a height thereof, such as at least a factor 5 larger.
  • a height of the nanoparticles is typically in the order of a crystallographic axis thereof, or a few times the axis, such as 1-50 nm or more.
  • the width and length of the nanoparticles are from 10 nm - 5 ⁇ m, preferably from 25 nm-1 ⁇ m, more preferably from 50 nm-500 nm, such as from 100 nm-250 nm.
  • the nanoparticles are suspended in the aqueous composition. Once a gel and/or glassy structure is formed it has been found that the nanoparticles are incorporated therein.
  • the present composition may comprise 0.5-80 wt.% solids, and water, preferably 1-50 wt.% solids, more preferably 1.5-30 wt.% solids, even more preferably 2-20 wt.% solids, such as 5-10 wt.% solids (based on a total weight of the composition).
  • the solids relate to biopolymer, and nanoparticles, and optionally to further additives.
  • the amount of bio-degradable polymer is (each individually) 1.5-80 wt.% (based on the total weight of the solids), preferably 2-40 wt.%, more preferably 3-30 wt.%, such as 5-20 wt.%.
  • the amount of nanoparticles is 0.01-80 wt.% (based on the total weight of the solids), preferably 0.1-70 wt.%, more preferably 1-60 wt.%, such as 5-50 wt.%. In other words the nanoparticles may form an abundant fraction of the solids, a very small fraction, or something in between.
  • the present invention relates to a solid composition, comprising 1.5-50 wt.% bio-degradable polymer, 0.01-80 wt.% nanoparticles, and less than 2 wt.% further additives.
  • a membrane is formed immediately, i.e. within a short time frame. As such properties of a surface are not changed significantly, e.g. by penetration of the composition or components thereof into the surface.
  • the present composition provides its beneficial effects thereto, without deterioration of the surface or optional underlying material.
  • setting thereof is controlled with the present membrane, typically without a need to provide (further) water, to control temperature, etc.
  • the process of setting can now be carried out without making use of huge amounts of (relatively) scarce resources, such as water, by providing a relatively cheap (amount of) composition forming a membrane.
  • a very important benefit of the present membrane is that it avoids drying of the concrete surface which drying, on its turn, might cause surface cracking. So (too much) drying of concrete involves cracking thereof. By providing the present membrane cracking is avoided. Apart from the reduction of permeability, prevention of cracking is a very important motivator to use the present membranes, also because it improves visual appearance of the concrete.
  • the present invention relates to a composition.
  • an amount (wt.%) of polymer is larger than an amount of nanoparticle.
  • the bio-degradable polymer is present in an amount of 1.5-64 wt.%, preferably 2-20 wt.%, more preferably 3-5 wt.%, based on a total weight of the composition.
  • the amount of polymer may be adjusted to e.g. ambient conditions, such as temperature, humidity, and to a surface to which the present composition may be applied, etc. If a flexible coating or membrane is required, an amount of polymer is higher, whereas if a stiff coating is required an amount of silicate may be higher. Depending on a type of polymer an amount may be higher, e.g. if a gel is somewhat difficult to form at low amounts thereof.
  • the amount is preferably 2-30 wt.%, more preferably 5- 20 wt.%, such as 10-15 wt.%. In general, these amounts provide the best characteristics. Also in view of applicability and viscosity the amounts may be varied.
  • the polyvalent cation is one or more of calcium, iron, copper, magnesium, strontium, aluminium, zinc, magnesium, and nickel, especially a M 2+ and M 3+ cation are preferred.
  • the cation is preferably non-toxic, such as calcium, iron, and magnesium, preferably calcium or iron.
  • the present invention can as a consequence in this respect be applied widely.
  • the nanoparticles are one or more of a natural or artificial clay, the clay preferably a monovalent cation clay.
  • the clay preferably has a cationic exchange capacity of 2-200 meq/100 grams clay at a pH of 7, more preferably 5-150 meq/100 grams, even more preferably 10-120 meq/100 grams. It has been found that clays having a relatively higher CEC perform better in terms of relevant characteristics for the present invention.
  • the clay may comprise one or more of H + , Na + , K + , Li + , and NH 4 +, .
  • the clay may be a tetrahedral-octahedral-tetrahedral (TOT)-clay (or 2:1 clay), such as a kaolin clay, such as kaolinite, dickite, halloysite and nacrite, a smectite clay, such as bentonite, montmorillonite, nontronite and saponite, an illite clay, a chlorite clay. Also a silicate mineral, such as mica, such as biotite, lepidolite, muscovite, phlogopite, zinnwaldite, clintonite, and allophane, are applicable as well as platelet like particles.
  • a clay applied may further be selected in view of required characteristics of a final coating. Addition of nanoparticles improves present characteristics, e.g. (decreased) permeability towards water, structural integrity, strength, flexibility, etc.
  • the nanoparticles are present in an amount of 0.01- 64 wt.%, preferably 0.1- 50 wt.%, more preferably 0.5- 30 wt.%, even more preferably 1- 20 wt.%, such as 2- 10 wt.% or 3-5 wt.%, based on a total weight of the composition. It is noted that relatively low amounts of nanoparticles may be used, which low amounts may still provide improved characteristics of the present invention. Higher amounts may be preferred, e.g. in view of (decreased) permeability, stiffness, integrity, etc.
  • composition may comprise further additives, such as an anti-fouling additive.
  • an anti-fouling additive such as CuSO 4 .
  • Additives may be added directly to the composition, if compatible, or may be added after applying the composition. Further additives, such as UV-blocker, stabilizers, fillers, colorants, and pigments may be added.
  • the present invention relates to a method of forming a bio-compatible membrane according to claim 1.
  • the present composition may be used, and similarly a first composition comprising the present polymer and a second composition comprising the present nanoparticles, if present, may be used.
  • the two compositions may be applied separately to a surface, and then mixing of the compositions may take place. As mixing may be less optimal in view of present characteristic of a coating being formed, application of one composition is typically preferred.
  • the present surface e.g. concrete, provides polyvalent cations, such as Ca 2+ . It has been found that a good coating is obtained by applying the present composition.
  • a (semi) solid surface like that of concrete is capable of providing polyvalent cations in sufficient amounts to form a membrane/coating according to the invention, and wherein the composition does not (or slightly at the most) penetrate the surface. Even further, without further measures the present method is capable of forming a membrane with required characteristics.
  • the present method may be repeated, e.g. if a thicker coating is required, if characteristics of the subsequent coating may or should vary, etc.
  • the surface is pre-treated and/or pre-shaped.
  • a surface can be given any (2- or 3-dimensional) shape.
  • the present coating applied to the surface inherently has a same (or at least similar) shape. If proper care is taken the present coating has exactly the same shape as the surface.
  • a surface may be used as a two- or three-dimensional mold. Very cheap reproductions may be made, having a very high quality.
  • the surface is one or more of concrete, cement material, and brick. These types of materials are widely used and formed and the present coating/membrane may provide advantageous characteristics to these materials.
  • the present biopolymer relates to so-called extracellular substances obtainable from granular sludge.
  • the extracellular polymeric substances comprise a major portion consisting of exopolysaccharides, and a minor portion, such as less than 30 % w/w, typically less than 10 %w/w, consisting of lipids and/or other components more hydrophobic than the exopolysaccharides.
  • weight percentages (w/w) throughout the description are based on a total weight of a (dry) composition.
  • Extracellular polymeric substances obtained from granular sludge having a major portion of exopolysaccharides and a minor portion of lipids have been found to provide very effective water resistance.
  • the extracellular polymeric substances comprise at least 50 % w/w exopolysaccharides, preferably at least 60 % w/w exopolysaccharides, most preferably at least 75 % w/w exopolysaccharides, such as at least 90 % w/w exopolysaccharides.
  • Extracellular polymeric substances obtained from granular sludge have been found to be particularly effective when they have a high exopolysaccharide content.
  • the exopolysaccharide content is preferably not 100 %, as the remainder has been found to contribute to the present advantageous effects.
  • the granular sludge is aerobic granular sludge or anammox granular sludge.
  • Extracellular polymeric substances obtained from aerobic granular sludge and anammox granular sludge have been shown to be particularly effective.
  • Research by the inventors has shown that exopolysaccharides of the extracellular polymeric substances obtained from aerobic granular sludge are alginate-like in character, and in fact perform even better than alginate per se.
  • Aerobic granular sludge and anammox granular sludge, and the processes used for obtaining them are known to a person skilled in the art.
  • the extracellular polymeric substances have been obtained from aerobic or anammox granular sludge by an isolation (i.e. separation) method comprising: alkaline extraction of the granular sludge thereby forming extracellular polymeric substances containing extractant; acid precipitation of extracellular polymeric substances from the extractant; and collecting the extracellular polymeric substance-containing precipitate.
  • the granular sludge has been substantially produced by bacteria belonging to the order Pseudomona-daceae, such as pseudomonas and/or Azotobacter bacteria (aerobic granular sludge); or, by bacteria belonging to the order Plancto-mycetales (anammox granular sludge), such as Brocadia anammoxidans, Kuenenia stuttgartiensis or Brocadia fulgida ; or, combinations thereof. Extracellular polymeric substances from granular sludge produced by these bacteria are effective.
  • Pseudomona-daceae such as pseudomonas and/or Azotobacter bacteria (aerobic granular sludge); or, by bacteria belonging to the order Plancto-mycetales (anammox granular sludge), such as Brocadia anammoxidans, Kuenenia stuttgartiensis or Brocadia fulgida ; or, combinations thereof.
  • the exopolysaccharides are blockcopolymers comprising uronic acid (e.g. mannuronic acid and guluronic acid) residues.
  • uronic acid e.g. mannuronic acid and guluronic acid
  • the clay is Na-montmorillonite.
  • the composition is applied in an amount of 10-1000 ml/m 2 , such as 10-500 ml/m 2 .
  • a relatively thin coating is sufficient to provide the present advantages.
  • a coating of 1-10 ⁇ m thickness is typically sufficient.
  • a sequence of coating layers may be applied.
  • a surface would be kept wet with water 1-30 l/m 2 would be required, i.e. at least an order of magnitude larger. Especially when (fresh) water is scarce and/or temperatures are high such may be an issue.
  • the composition is applied at least once by one or more of spraying, brushing, nebulizing, and pouring.
  • the present method is relatively insensitive to a way application is performed. For some surfaces, especially ones less accessible, spraying/nebulizing is preferred.
  • the composition is applied directly after casting cement or concrete.
  • the present invention relates to a method of protecting a surface from degradation. As indicated throughout the application especially these materials are considered.
  • the surface is protected from one or more of drying, oxidizing, such as corroding, wearing, fouling, and dehydrating.
  • the present invention relates to a method of forming a coating.
  • the coating is flexible. It is noted that combinations of polymers may be used, as well as combinations of nanoparticles, in order to obtain required characteristics.
  • the coating has a thickness of 5-500 ⁇ m, more preferably a thickness of 10-250 ⁇ m, such as a thickness of 50-100 ⁇ m.
  • a relatively thicker coating e.g. 100 ⁇ m
  • a low amount of composition 0.1 l/m 2
  • the present invention relates to a use of the present composition and/or of the present flexible polymer coating for one or more of improving setting of concrete, protecting concrete or cement material from degradation.
  • the water-vapor transmission on an example of the present membrane was determined gravimetrically by a water-vapor permeability test, which was performed using a cup method, according to ASTM E96.
  • the water vapor permeability was found to be 1.8 * 10 -10 g/smPa. Typical values found are 1-10*10 -10 g/smPa.
  • the aerobic granular sludge from which the extracellular polymeric substances of the present example were obtained was collected from the Nereda ® pilot plant, operated by DHV at the wastewater treatment plant Epe, The Netherlands.
  • the reactor was fed with municipal sewage.
  • the influent consisted of approximately 25% of slaughterhouse wastewater, which was discharged in the sewage system. Average parameters of the influent were: CODtotal 585 mg/L, suspended solids 195 mg/L, NH 4 -N 55 mg/L and PO4-P 6.3 mg/L.
  • the reactor was operated in Sequencing Batch (SBR) mode for biological phosphate and nitrogen removal. Operational details were described in Lin et al. (2010). After start-up, biomass concentration in the reactor was maintained around 8 to 10 g TSS/L.
  • Oxygen in the reactor was controlled between 2 to 3 mg/L during aeration. Temperature and pH were not controlled in this system and depended on the incoming sewage. During steady operation, aerobic granular sludge was collected and sieved to give granules with a diameter > 2 mm.
  • the granules were then dried.
  • Dried granules (0.5 g) were homogenized for 5 min (Labgen tissue homogenizer, Cole-Parmer, USA) and extracted in 80 ml 0.2 M Na 2 CO 3 at 80 °C for 1 h. After centrifuging at 15,000 rpm for 20 min, the pellet was discarded. The supernatant pH was adjusted to 2 by adding 0.1 M HCl. The precipitate was collected by centrifugation (15,000 rpm, 30 min), washed by di-deionized water until effluent pH reached 7, and dissolved in 0.1 M NaOH. Extracellular polymeric substances in the supernatant were precipitated by the addition of cold absolute ethanol to a final concentration of 80% (vol/vol).
  • the precipitate was collected by centrifugation (15,000 rpm, 30 min), washed three times in absolute ethanol and lyophilized.
  • the resulting mixture of extracellular polymer substances is an example of extracellular polymeric substances (EPS) obtainable from granular sludge according to the invention.
  • Ash content of the EPS was measured according to the standard method (APHA).
  • EPS 0.5 g was dissolved in 15 mL of NaOH solution (0.05 M). The pH was then adjusted to 7.0 by 0.05 M HCl. Finally the solution was placed inside a dialysis tubing (3500 MWCO) and dialyzed against demineralized water for 48 hours to remove loosely bound ions and lyophilized.
  • Imaging of EPS was carried out in air at ambient temperature and humidity using freshly-cleaved mica pre-treated by 3 mM NiCl 3 . Aliquots (2ul) of extracellular polymeric substances (5 mg/L) were deposited onto mica surfaces for 10 s, and then quickly removed by the pipette. Those surfaces were air dried (1h) in a dust-free enclosure. Samples were scanned with a Digital Instruments Multimode atomic force microscope (Veeco nanoscopy iva dimension 3100, Veeco Inc., Santa Barbara, USA).
  • Pyrolysis was carried out on a Horizon Instruments Curie-Point pyrolyser.
  • the lyophilized extracellular polymeric substances were heated for 5 s at 600°C.
  • the pyrolysis unit was connected to a Carlo Erba GC8060 gas chromatograph and the products were separated by a fused silica column (Varian, 25 m, 0.25 mm i.d.) coated with CP-Sil5 (film thickness 0.40 ⁇ m). Helium was used as carrier gas.
  • the oven was initially kept at 40°C for 1 min, next it was heated at a rate of 7°C/min to 320°C and maintained at that temperature for 15 min.
  • the column was coupled to a Fisons MD800 mass spectrometer (mass range m/z 45-650, ionization energy 70 eV, cycle time 0.7 s). Identification of the compounds was carried out by their mass spectra using a NIST library or by interpretation of the spectra, by their retention times and/or by comparison with literature data.
  • One milliliter of the organic phase was filtered over water-free sodium sulphate into GC vials.
  • the lipids in the organic phase were analyzed by gas chromatography (model 6890N, Agilent, USA) equipped with a FID, on an HP Innowax column.
  • Size exclusion chromatography was performed with a Superdex 75 10/300 GL column (AKTA Purifier System, GE Healthcare). Elution was carried out at room temperature using PBS at constant 0.4 mL/min flow rate and detection was monitored by following the absorbance of the eluted molecules at 210 nm.
  • EPS (1 g) was put into H 2 O 2 (30%) for 24 hours, collected by centrifuge at 4000 rpm and lyophilized. Morphology of Extracellular polymeric substances by the atomic force microscope
  • the yield of extracellular polymeric substances was 160 ⁇ 4 mg/g (VSS ratio).
  • the extracellular polymeric substances have a fiber-like structure.
  • the width of the fiber is around 20 nm.
  • the fibers extend along the surface and entangle with each other, forming a web-like structure that covers the whole surface of the mica. This demonstrates that the extracellular polymeric substances have a perfect film-forming property and can form a continuous film on a surface.
  • the thickness of extracellular polymeric substance film is around 4 nm.
  • the globules looked much brighter than the fibers under the atomic force microscope.
  • the sample was prepared by depositing extracellular polymeric substance water solution on a surface and air dried, those globules extending out of the surface and pointing to the air must have hydrophobic property.
  • the extracellular polymeric substances have both a hydrophilic part and hydrophobic part.
  • the hydrophilic parts spread along the surface, forming a film and the hydrophobic parts distribute on the film and pointing to the air.
  • the composition of the extracellular polymeric substances was analyzed by pyrolysis-GC-MS.
  • polysaccharide-derived products such as 5-methylfuraldhyde and levoglucosenone were identified, implying a contribution from carbohydrate units to the extracellular polymeric substance sample.
  • Lipids and wax esters composed of C 16 and C 18 fatty acids and alcohol moieties of the same carbon lengths were found as well.
  • all pyrolysis products of proteins and other combinations of amino acids were much less prominent, indicating that they were relatively minor components of the extracellular polymeric substances.
  • there is a so-called unresolved complex mixture consisting of many similar compounds that co-elute and which cannot be identified by their mass spectra at present.
  • the pyrolysis-GC-MS analysis displays that, comparing to carbohydrates and lipids, proteins are a minor part of the extracellular polymeric substances.
  • the lipid content in the extracellular polymeric substances was measured as 8.2 ⁇ 0.9 mg/g extracellular polymeric substances.
  • the size distribution profile of the extracellular polymeric substances by size exclusion chromatography is determined. There are 5 fractions with different elution volume. The fraction with the shortest elution volume, which has the highest molecular weight, separate well with other fractions. The three fractions with an elution volume between 13 ml to 17 ml co-eluted. The molecular weight of these 5 fractions and their percentages are listed in Table 1. It can be clearly seen that most of isolated extracellular polymeric substances (94%) has a molecular weight of more than 5.8 KDa, and about 1/3 of the extracellular polymeric substances has a molecular weight higher than 150 KDa.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Paints Or Removers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Claims (9)

  1. Procédé de formation d'une membrane biocompatible comprenant les étapes suivantes
    fournir une composition comprenant (i) de l'eau, (ii) un polymère biodégradable anionique soluble dans l'eau et (iii) des nanoparticules de plaquettes, soit en tant que telles, soit en parties de celles-ci,
    dans laquelle le polymère biodégradable est en une quantité de 1,5-64 % en poids, sur la base du poids total de la composition, dans laquelle le biopolymère est un exopolysaccharide de type alginate de substances polymères extracellulaires obtenu à partir de boues granulaires aérobies ou annamiques et n'est pas un alginate en soi,
    dans laquelle les nanoparticules sont en une quantité de 0,01 à 64 % en poids, par rapport à un poids total de la composition, dans laquelle les nanoparticules sont de l'argile,
    l'application de la composition sur une surface, la surface fournissant des cations polyvalents, faire réagir le polymère biodégradable (ii)(a) et les cations polyvalents, formant ainsi une couche de membrane sur la surface.
  2. Procédé selon la revendication 1, dans lequel la surface est prétraitée et/ou préformée.
  3. Procédé selon une ou plusieurs des revendications précédentes, dans lequel la surface est un ou plusieurs des matériaux suivants: béton, ciment, et brique.
  4. Procédé selon l'une quelconque des revendications précédentes, dans lequel la composition est appliquée au moins une fois par une ou plusieurs des méthodes suivantes: pulvérisation, brossage, nébulisation, et coulée, et
    dans lequel la composition est appliquée directement après le coulage du ciment ou du béton.
  5. Procédé de protection d'une surface contre la dégradation par la mise en oeuvre d'un procédé selon l'une quelconque des revendications précédentes, tel que
    dans lequel la surface est protégée contre un ou plusieurs des phénomènes suivants:
    séchage, oxydation, telle que la corrosion, usure, encrassement, et déshydratation.
  6. Composition aqueuse pour former une membrane biocompatible comprenant
    (i) de l'eau,
    (ii) un polymère biodégradable anionique soluble dans l'eau, dans lequel le polymère est capable de former un gel au contact de cations polyvalents dans des conditions ambiantes, le polymère étant dissous dans le liquide, dans lequel le biopolymère est un exopolysaccharide de type alginate de substances polymères extracellulaires obtenues à partir de boues granulaires aérobies ou annamiques et n'est pas un alginate en soi et
    (iii) des nanoparticules de plaquettes, les nanoparticules étant en suspension dans le liquide,
    dans lequel le polymère biodégradable est présent en une quantité de 1,5 à 64 % en poids, sur la base du poids total de la composition,
    dans lequel les nanoparticules sont présentes en une quantité de 0,01 à 64 % en poids, sur la base du poids total de la composition, dans lequel les nanoparticules sont de l'argile.
  7. Composition selon la revendication 6, dans laquelle
    une quantité (% en poids) de polymère est supérieure à une quantité de nanoparticules.
  8. Composition selon l'une ou plusieurs des revendications 6 à 7, dans laquelle les nanoparticules sont présentes en une quantité de 0,1 à 50 % en poids, par rapport à un poids total de la composition.
  9. Utilisation d'une composition selon l'une quelconque des revendications 6 à 8 pour un ou plusieurs des usages suivants: amélioration de la prise du béton, protection du béton ou du matériau cimentaire contre la dégradation, et comme revêtement anti-graffiti.
EP14790758.8A 2013-10-03 2014-10-03 Composition pour la formation d'une membrane à base biologique, procede d'application sur des surfaces et utilisation de celle-ci Active EP3052223B1 (fr)

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WO2015050449A2 (fr) 2015-04-09
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EP3052223A2 (fr) 2016-08-10
IL244865A0 (en) 2016-05-31
NL2011542B3 (en) 2024-02-28
WO2015050449A3 (fr) 2015-05-28
US10570304B2 (en) 2020-02-25
US20160251533A1 (en) 2016-09-01
PT3052223T (pt) 2022-03-09
NL2011542C2 (en) 2015-04-07

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